CN109943913B - Soft moisture-absorbing and easy-to-dye crimped fiber and preparation method thereof - Google Patents
Soft moisture-absorbing and easy-to-dye crimped fiber and preparation method thereof Download PDFInfo
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Abstract
The invention provides a soft moisture-absorption easily-dyed crimped fiber and a preparation method thereof, wherein the soft moisture-absorption easily-dyed crimped fiber comprises the following components in percentage by mass: polyamide 5X 10-50% and polyester 50-90%. The invention can obtain the fiber which is easy to dye by using the acid dye and the disperse dye at low temperature with lower cost and simple working procedures.
Description
Technical Field
The invention relates to a fiber technology, in particular to a soft moisture-absorption easily-dyed crimped fiber and a preparation method thereof, belonging to the technical field of spinning.
Background
The polyester fiber has the advantages of high stiffness, high strength, high modulus, solvent resistance, heat resistance, fatigue resistance and the like, and is widely applied to civil and industrial materials. However, polyester fiber as a textile material has some disadvantages, mainly because polyester macromolecular chains are closely arranged, crystallinity and orientation degree are high, and polar groups are lacking in the molecular chains, so that the prepared fiber has poor softness, hygroscopicity and dyeability, static electricity is easy to generate, the fabric is easy to pilling, and the polyester fiber has poor wear resistance.
Because polyester has high crystallinity and a molecular chain is lack of polar groups, fibers prepared from the polyester fibers generally need to be dyed by disperse dyes and need to be dyed under the conditions of high temperature and high pressure, and the high-temperature and high-pressure operation is generally dangerous, has higher requirements on dyeing equipment and wastes energy.
At present, in order to overcome some defects of polyester fibers, physical and chemical methods are mainly adopted to modify polyester. The chemical method comprises the following steps: copolymerization and surface treatment are adopted to change the chemical structure of the original polyester macromolecules so as to improve the performance of the fiber. Physical method: under the condition of not changing the chemical structure of polyester macromolecule, the purpose of improving the fiber performance is achieved by changing the morphological structure of the fiber, such as composite spinning, blend spinning, anisotropic spinning or fiber mixing and interweaving, and the fiber which is easy to dye, highly hygroscopic, antistatic and soft is prepared.
For example, patent CN103757745B discloses a polyester blend fiber and a preparation method thereof, which adopts blend spinning of modified polyester and polyamide, the selected modified polyester is chemically modified in polymerization, the molecular chain structure is seriously damaged, the selected blend material is polyamide 6 and polyamide 66, the blend fiber is prepared by adopting a copolymerization and blending method, the operation is complicated, and the production cost investment is increased; patent CN105040156A discloses a blend fiber, its preparation method and fabric containing the blend fiber, the blend fiber comprises polyamide with a content of 1-40 weight parts, and polyester with a content of 60-99 weight parts, the blend fiber is spun by blending with slice, the breaking strength of the blend fiber is 1.5-5.5 cN/dtex. CN 103233283B discloses a method for manufacturing a high-strength high-elongation polyester tire cord, cord precursor and a cord, wherein the cord precursor is prepared by blending and spinning two polymers, the component A is polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate and modified polyethylene terephthalate, the content of the component A is 90-95 wt%, the component B is polyamide, and the content of the component B is 5-10 wt%. The blending spinning method has the defect of uneven melt mixing, the two components are thermodynamically incompatible polymer systems, and the blending spinning method is adopted, so that crystallization-induced phase separation is easy to occur due to asynchronous crystallization in the cooling process of the two polymer melts out of a spinneret plate, the mechanical property of the material is reduced, and the uneven elongation rate of fibers is increased;
CN 102154716A discloses a co-spinning method of polyamide-polyester industrial yarn, and provides a method for preparing the polyamide-polyester industrial yarn by a co-spinning method, wherein the center of the polyamide-polyester industrial yarn is polyester, and the center of the polyamide-polyester industrial yarn is completely wrapped by peripheral polyamide 6 (polyamide 6). Wherein, the terylene accounts for 15 to 30 weight percent and the chinlon accounts for 85 to 70 weight percent. The strength reaches 8.2-8.7cN/dtex, the modulus reaches 60-85 wt%, and the elongation at break reaches 10-15%. The spinning forming conditions of terylene and chinlon 6 are different, the spinning tension of chinlon 6 is high, the tension is not easy to control when the chinlon 6 is co-spun with polyester, chinlon 6 is easy to crystallize, and the phenomenon of edge collapse is easy to generate due to improper control of the spinning speed during winding, so that the full-winding rate is reduced.
At present, polyamide 6/polyester sheath-core composite fiber is mainly used, polyamide 6 is mainly used to obtain good dyeing property, hygroscopicity and wear resistance, and terylene is used as a core to obtain better elastic modulus, so that the defect that chinlon is easy to deform and wrinkle is overcome.
There is no report on polyamide 5X/polyester sheath-core composite fibers.
Disclosure of Invention
In order to solve the defects of poor fiber softness, low moisture absorption rate, poor dyeing property and the like, the invention provides the soft moisture-absorption easy-to-dye crimped fiber and the preparation method thereof.
The invention provides a soft moisture-absorption easily-dyed crimped fiber which comprises the following components in percentage by mass: polyamide 5X 10-50% and polyester 50-90%.
Wherein, the polyamide 5X can be generated by polymerizing 1, 5-pentanediamine and dibasic acid, and the 1, 5-pentanediamine and the dibasic acid can be prepared from biological base materials by a fermentation method or an enzyme conversion method in order to reduce environmental pollution.
Wherein the dibasic acid comprises a C6-20 aliphatic dibasic acid, namely: the number of carbon atoms of the aliphatic dibasic acid is more than or equal to 6, preferably 8-20, and more preferably 10-16; specifically, the dibasic acids include: adipic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, maleic acid and Δ 9-1, 18-octadecenedioic acid.
In the preparation of polyamide 5X, the starting materials for the preparation may be selected from comonomers and/or additives in addition to the abovementioned 1, 5-pentanediamine and dibasic acid.
Wherein the comonomer is selected from one or more of aliphatic dicarboxylic acid, alicyclic dicarboxylic acid, aromatic dicarboxylic acid, ethylenediamine, hexamethylenediamine, cyclohexanediamine, xylylenediamine, 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid, p-aminomethylbenzoic acid, epsilon-caprolactam and omega-laurolactam;
the additive is selected from one or more of antistatic agent, delustering agent, flame retardant, antioxidant, ultraviolet absorbent, infrared absorbent, crystallization nucleating agent, fluorescent whitening agent and antistatic agent; wherein the additive accounts for 0.001-10% of the total weight of the raw materials.
The fiber prepared by the composition has the characteristics of softness, easy moisture absorption, easy dyeing and easy curling, and when the acid dye and the disperse dye are used for dyeing, the dyeing process does not need high temperature and high pressure, and the operation difficulty is low. Therefore, the fiber of the invention can be applied to civil and industrial aspects, such as socks, underwear, shirts, sweaters, carpets and the like, and industrial aspects such as sewing threads, fishing nets, cables and the like.
The soft moisture absorption easily-dyed crimped fiber is of a sheath-core structure, wherein the sheath-core structure comprises a positive core structure and a core shift structure.
Further, the sheath-core structure is preferably an eccentric core structure.
In the skin-core structure, the polyamide is a skin layer material, and the polyester is a core layer material. The content of the skin layer material is preferably 15 to 45%, more preferably 20 to 40%, and the content of the core layer material is preferably 55 to 85%, more preferably 60 to 80%.
In addition, the cross section shape of the soft moisture absorption dyeable crimped fiber is not particularly limited, and can be any one of a circle, a trefoil, a cross, a triangle, a hollow triangle, an I shape, a T shape, a Y shape, a flat shape, a pentagon, a hexagon, an octagon, an I shape or a dumbbell shape.
Further, the polyamide 5X in the present invention is selected from one or more of polyamide 56, polyamide 510 or polyamide 512;
the polyester is selected from one or more of polyethylene terephthalate, polytrimethylene terephthalate and polybutylene terephthalate, and is preferably polyethylene terephthalate.
The titer of the soft moisture-absorption easy-dyeing crimped fiber is 10-1000dtex, preferably 50-500dtex, more preferably 70-300dtex, more preferably 90-200dtex, and more preferably 120-150 dtex;
the breaking strength of the soft moisture absorption dyeable crimped fiber is 2.5-7.0cN/dtex, preferably 3.0-6.5cN/dtex, more preferably 3.5-6.0cN/dtex, and even more preferably 4.0-5.5 cN/dtex;
the breaking elongation of the soft hygroscopic easily-dyed crimped fiber is 20-60%, preferably 25-55%, more preferably 30-50%, and still more preferably 35-45%;
the initial modulus of the soft moisture absorption dyeable crimped fiber is 20-70cN/dtex, preferably 25-65cN/dtex, more preferably 30-60cN/dtex, and more preferably 35-55 cN/dtex;
the moisture regain of the soft hygroscopic and dyeable crimped fiber is 1.0 to 3.0%, preferably 1.2 to 2.8%, more preferably 1.5 to 2.5%, and still more preferably 1.8 to 2.2%;
the untreated elastic recovery rate of the soft hygroscopic easily-dyed crimped fiber is 85-100%, preferably 87-98%, more preferably 89-96%, and still more preferably 92-94%;
the elastic recovery rate of the soft hygroscopic easy-dyeing crimped fiber after treatment is 85-100%, preferably 87-98%, more preferably 90-96%, and still more preferably 93-94%;
in addition, the soft hygroscopic easy-dyeing crimped fiber is easy to dye, especially is easy to dye acid dyes and disperse dyes, wherein the dyeing rate of the acid dyes is 70-100%, preferably 73-98%, more preferably 78-92%, even more preferably 82-88%, and the dyeing temperature of the acid dyes is 50-90 ℃, preferably 55-85 ℃, more preferably 60-80 ℃, even more preferably 65-75 ℃; the dyeing uptake of the disperse dye is 85-100%, preferably 88-98%, more preferably 90-97%, and still more preferably 92-94%, and the dyeing temperature of the disperse dye is 80-130 ℃, preferably 85-125 ℃, more preferably 90-120 ℃, and still more preferably 100-110 ℃.
The invention also provides a preparation method of any one of the soft moisture-absorption and easy-dyeing crimped fibers, which comprises the following steps:
1) the polyamide 5X melt and the polyester melt are converged in a composite spinning assembly, sprayed out through a spinneret plate of a spinning manifold, and cooled to generate a primary yarn;
2) carrying out post-treatment on the as-spun yarn to obtain the soft moisture-absorbing and easily-dyed crimped fiber;
wherein the post-treatment comprises stretching treatment, the temperature of the stretching treatment is 50-200 ℃, the stretching treatment is at least two-stage stretching, and the total stretching multiple of the stretching treatment is 1.5-5.0.
In the step 1), the polyamide 5X melt and the polyester melt are merged in the composite spinning assembly, specifically, the polyamide 5X melt and the polyester melt are merged in the composite spinning assembly through respective melt pipelines.
In addition, the polyamide 5X melt in the step 1) can be subjected to polycondensation reaction and hot melting of the 1, 5-pentanediamine and the dibasic acid to obtain a polyamide 5X melt; the polyamide 5X resin may also be heated to a molten state by a screw extruder to obtain a polyamide 5X melt. When the polyamide 5X melt is prepared by direct hot melting of a polyamide 5X resin by a screw extruder, the polyamide 5X resin has a relative viscosity at 96 wt% sulfuric acid of 2.0 to 4.0, preferably 2.4 to 3.5, more preferably 2.7 to 3.0; the water content of the polyamide 5X resin is 50-1000ppm, preferably 200-800ppm, more preferably 300-700ppm, and further preferably 400-600 ppm.
The method for preparing the polyamide 5X melt by directly polymerizing 1, 5-pentanediamine and dibasic acid comprises the following steps: under the condition of nitrogen, 1, 5-pentanediamine, dicarboxylic acid and water are uniformly mixed to prepare a salt solution of polyamide 5X; wherein the molar ratio of the 1, 5-pentanediamine to the dicarboxylic acid is (1-1.2): 1; then heating the salt solution of polyamide 5X, raising the pressure in the reaction system to 0.3-2.5MPa, exhausting, maintaining the pressure, reducing the pressure to gauge pressure of 0-0.3MPa, and vacuumizing to the vacuum degree of-0.08 to-0.01 MPa to obtain a polyamide 5X melt; in the reaction process, the temperature of the reaction system is 230-275 ℃ after the pressure maintaining is finished, the temperature of the reaction system is 245-285 ℃ after the pressure reduction is finished, and the temperature after the vacuum pumping is 250-280 ℃.
In addition, in addition to the above method, the preparation of polyamide 5X can also be accomplished by adding monomers and additives, the preparation method comprising: under the condition of nitrogen, 1, 5-pentanediamine, dicarboxylic acid, caprolactam and water are uniformly mixed to prepare a salt solution of polyamide 5X, and a fluorescent whitening agent is added; wherein the molar ratio of the 1, 5-pentanediamine to the dicarboxylic acid is (1-1.08): 1, wherein the mass of the fluorescent whitening agent accounts for 0.3 wt% of the total reactant mass, and the mass of the caprolactam accounts for 3 wt% of the total reactant mass; then heating the salt solution of polyamide 5X, raising the pressure in the reaction system to 0.25-2.3MPa, exhausting, maintaining the pressure, reducing the pressure to gauge pressure of 0-0.35MPa, and vacuumizing to the vacuum degree of-0.08 to-0.01 MPa to obtain a polyamide 5X melt; in the reaction process, the temperature of the reaction system is 232-.
Similarly, the polyester melt in step 1) can be prepared by polymerizing and hot-melting terephthalic acid and a dihydric alcohol selected from ethylene glycol, propylene glycol and butanediol, and correspondingly preparing polyethylene terephthalate, polytrimethylene terephthalate and polybutylene terephthalate respectively; the polyester resin can also be directly heated to a molten state through a screw extruder to obtain a polyester melt. When the polyester resin is selected and directly hot-melted by a screw extruder to prepare the polyester melt, the inherent viscosity of the polyester is 0.6-1.1dL/g, preferably 0.7-1.0dL/g, and more preferably 0.8-0.9 dL/g; the water content of the polyester resin is 20 to 150ppm, preferably 30 to 100ppm, more preferably 40 to 80ppm, and further preferably 50 to 60 ppm.
In addition, in the step 1), after the polyamide 5X melt and the polyester melt are sprayed out through a spinneret plate of a spinning manifold, the raw silk can be generated only through cooling treatment. The cooling treatment is cross-air blow cooling, the air speed of the cross-air blow is 0.5-1.3m/s, preferably 0.7-1.1m/s, the temperature of the cross-air blow is 14-30 ℃, preferably 18-28 ℃, the humidity of the cross-air blow is 60-80%, preferably 65-75%
The post-treatment of the primary raw silk in the step 2) sequentially comprises oiling treatment, stretching treatment, heat setting treatment and winding treatment. Among them, the stretching treatment, the winding treatment, and the heat-setting treatment are very important.
The drawing treatment specifically means drawing the as-spun yarn to a target length. In the invention, when the fiber is prepared, the drawing treatment of the primary yarn is at least two-stage drawing, namely at least two times of drawing. That is, three-stage stretching, four-stage stretching, five-stage stretching, or six-stage stretching may be performed. The temperature of the stretching treatment is 50 to 200 ℃ at the time of the stretching treatment, and the total stretching ratio is 1.5 to 5 times, that is, when the stretching treatment is completed, the length after the stretching is 1.5 to 5 times the length before the stretching.
In addition, the speed of the winding treatment is 2000-5500m/min, preferably 2500-50000m/min, and more preferably 3000-35000 m/min; the temperature of the heat setting is 100-200 ℃, preferably 130-180 ℃. The temperature of the heat setting treatment is 100-200 ℃, preferably 130-180 ℃.
In step 1), when the polyamide 5X melt is prepared by first heat treatment of a polyamide 5X resin by a first screw extruder, in order to make the fiber prepared by the present invention have the characteristics of softness, easy moisture absorption, easy dyeing and easy curling, the operating parameters of the first screw extruder during the first heat treatment can be further defined, specifically: setting the first screw extruder as a five-zone heating mode, wherein the temperature of the first zone is 200-; when the polyester melt is prepared by performing the second heat treatment on the polyester through the second screw extruder, the working parameters of the second screw extruder during the second heat treatment can be further defined, specifically: the first screw extruder is set to be in a five-zone heating mode, wherein the temperature of the first zone is 200-.
When the first screw extruder and the second screw extruder meet the conditions, the temperature of the second zone can be further limited to be higher than the temperature of the first zone, and the temperature of the third zone, the temperature of the fourth zone and the temperature of the fifth zone are respectively higher than the temperature of the first zone and/or the temperature of the second zone.
It is to be noted that the first screw extruder and the second screw extruder in the present invention may be the same or different, wherein "first" and "second" are only used to distinguish the separate operations for polyamide 5X and polyester.
Further, the temperature of the spinning box body is 220-320 ℃, and the pressure of the composite spinning assembly is 10-30 MPa.
The implementation of the invention has at least the following advantages:
1. the fiber of the invention has the characteristics of softness, easy moisture absorption, easy dyeability at low temperature, three-dimensional curling and high elasticity, thereby overcoming the outstanding defects of the prior fiber;
2. the preparation method of the invention selects polyamide 5X with melting point and crystallization temperature similar to polyester to carry out skin-core structure, which accords with spinning, and does not generate phase separation phenomenon in the process of blending spinning;
3. the preparation method of the fiber is simple and easy to operate, does not need large-scale equipment for assistance, has low production cost and is suitable for industrial production;
4. the polyamide 5X resin selected by the invention is prepared by a biological method, is a green material, does not depend on petroleum resources, does not cause serious pollution to the environment, can reduce the emission of carbon, and is beneficial to reducing the generation of greenhouse effect.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the soft hygroscopic easy-to-dye crimped fiber of the embodiment is as follows:
1) the polyamide 56 melt and the polyethylene glycol terephthalate melt are converged in a composite spinning assembly in a spinning manifold through respective melt pipelines, sprayed out through an eccentric composite spinneret plate, and cooled to form primary yarns;
wherein, the proportion of the sheath-core components is accurately adjusted by a metering pump, the content of polyamide 56 in the sheath layer is 20 wt%, and the content of polyethylene terephthalate in the core layer is 80 wt%;
wherein the temperature of the spinning manifold is 285 ℃, and the pressure of the spinning assembly of the spinning manifold is 15 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain soft moisture-absorbing and easily-dyed crimped fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.6m/s, the temperature of the side-blown air is 24 ℃, and the humidity of the side-blown air is 70%;
the post-treatment comprises the following steps: and performing oiling treatment, stretching treatment, heat setting treatment and winding treatment on the as-spun yarn. The stretching treatment is secondary stretching, the total stretching multiple is 3.0 times, and the stretching temperature is 80 ℃; the temperature during the heat setting treatment was 210 ℃ and the winding speed was 3800 m/min.
The preparation method of the melt of polyamide 56 in this example was: drying polyamide 56 resin (96% sulfuric acid with relative viscosity of 2.7 and water content of 400ppm) in a vacuum drum dryer at 110 ℃ for 15h, and heating to a molten state by using a first screw extruder to form a polyamide 56 melt; wherein the first screw extruder is heated in five zones, the temperature of the first zone is 240 ℃, the temperature of the second zone is 250 ℃, the temperature of the third zone is 260 ℃, the temperature of the fourth zone is 270 ℃, and the temperature of the fifth zone is 280 ℃.
The preparation method of the polyethylene terephthalate melt in this example was: drying polyethylene terephthalate resin (with intrinsic viscosity of 0.67dL/g and water content of 60ppm) in a continuous hot air drying tower at 150 ℃ for 24h, and heating to a molten state by using a second screw extruder to form a polyethylene terephthalate melt; wherein the second screw extruder is heated in five zones, the temperature of the first zone is 250 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 285 ℃.
In this example, the relative viscosity of polyamide 5X was measured as follows:
concentrated sulfuric acid method by Ubbelohde viscometer: accurately weighing 0.25 + -0.0002 g of dried polyamide 5X slice or staple fiber sample thereof, adding 50mL of concentrated sulfuric acid (96%) for dissolution, measuring and recording the flowing time t of the concentrated sulfuric acid in a constant-temperature water bath at 25 DEG C0And the polyamide sample solution flowing time t.
Viscosity number calculation formula: relative viscosity t/t0
t-solution flow time;
t0-solvent flow time.
The intrinsic viscosity was measured as follows:
solvent: phenol-tetrachloroethane (1:1) according to GB/T14901993 fibre grade polyester chip analysis method. Intrinsic viscosity ((1+1.4(t/t0-1))0.5-1)/0.7c (unit dL/g), t is the flow-out time of the solution, and t is0As solventsThe flow-out time, c, is the solution concentration.
Example 2
The preparation method of the soft hygroscopic easy-to-dye crimped fiber of the embodiment is as follows:
1) the polyamide 56 melt and the polytrimethylene terephthalate melt are converged in a composite spinning assembly in a spinning manifold through respective melt pipelines, sprayed out through an eccentric composite spinneret plate, and cooled to form a primary raw yarn;
wherein, the proportion of the sheath-core components is accurately adjusted by a metering pump, the content of polyamide 56 in the sheath layer is 30 wt%, and the content of polyethylene terephthalate in the core layer is 70 wt%;
wherein the temperature of the spinning beam is 290 ℃, and the pressure of the spinning assembly of the spinning beam is 17 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain soft moisture-absorbing and easily-dyed crimped fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.5m/s, the temperature of the side-blown air is 23 ℃, and the humidity of the side-blown air is 75%.
The post-treatment comprises the following steps: and performing oiling treatment, stretching treatment, heat setting treatment and winding treatment on the as-spun yarn. The stretching treatment is secondary stretching, the total stretching multiple is 3.5 times, and the stretching temperature is 70 ℃; the temperature during the heat-setting treatment was 200 ℃ and the winding speed was 4500 m/min.
The preparation method of the melt of polyamide 56 in this example was: drying polyamide 56 resin (96% sulfuric acid with relative viscosity of 2.8 and water content of 300ppm) in a vacuum drum dryer at 105 ℃ for 20h, and heating to a molten state by using a first screw extruder to form a polyamide 56 melt; wherein the first screw extruder is heated in five zones, the temperature of the first zone is 245 ℃, the temperature of the second zone is 255 ℃, the temperature of the third zone is 265 ℃, the temperature of the fourth zone is 275 ℃, and the temperature of the fifth zone is 285 ℃.
The preparation method of the polytrimethylene terephthalate melt in this example was: drying polytrimethylene terephthalate resin (with intrinsic viscosity of 1.0dL/g and water content of 50ppm) in a continuous hot air drying tower at the drying temperature of 120 ℃ for 30h, and then heating to a molten state by using a second screw extruder to form polytrimethylene terephthalate melt; wherein the second screw extruder is heated in five zones, the temperature of the first zone is 255 ℃, the temperature of the second zone is 275 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 295 ℃, and the temperature of the fifth zone is 290 ℃.
The relative viscosity and intrinsic viscosity were measured as described in example 1.
Example 3
The preparation method of the soft hygroscopic easy-to-dye crimped fiber of the embodiment is as follows:
1) the polyamide 56 melt and the polyethylene glycol terephthalate melt are converged in a composite spinning assembly in a spinning manifold through respective melt pipelines, sprayed out through a positive core composite spinneret plate, and cooled to form primary raw silk;
wherein, the proportion of the sheath-core components is accurately adjusted by a metering pump, the content of polyamide 56 in the sheath layer is 50 wt%, and the content of polyethylene terephthalate in the core layer is 50 wt%;
wherein the temperature of the spinning manifold is 292 ℃, and the pressure of the spinning assembly of the spinning manifold is 16 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain soft moisture-absorbing and easily-dyed crimped fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.8m/s, the temperature of the side-blown air is 22 ℃, and the humidity of the side-blown air is 68 percent
The post-treatment comprises the following steps: and performing oiling treatment, stretching treatment, heat setting treatment and winding treatment on the as-spun yarn. The stretching treatment is secondary stretching, the total stretching multiple is 3.8 times, and the stretching temperature is 70 ℃; the temperature during the heat setting treatment was 190 ℃ and the winding speed was 4800 m/min.
The preparation method of the melt of polyamide 56 in this example was: drying polyamide 56 resin (96% sulfuric acid with relative viscosity of 2.5 and water content of 500ppm) in a vacuum drum dryer at 100 ℃ for 25h, and heating to a molten state by using a first screw extruder to form a polyamide 56 melt; wherein the first screw extruder is heated in five zones, the temperature of the first zone is 242 ℃, the temperature of the second zone is 256 ℃, the temperature of the third zone is 268 ℃, the temperature of the fourth zone is 276 ℃, and the temperature of the fifth zone is 288 ℃.
The preparation method of the polyethylene terephthalate melt in this example was: drying polyethylene terephthalate resin (with intrinsic viscosity of 0.68dL/g and water content of 40ppm) in a continuous hot air drying tower at 155 ℃ for 20h, and heating to a molten state by using a second screw extruder to form a polyethylene terephthalate melt; wherein the second screw extruder is heated in five zones, the temperature of the first zone is 255 ℃, the temperature of the second zone is 278 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 295 ℃.
The relative viscosity and intrinsic viscosity were measured as described in example 1.
Example 4
The preparation method of the soft hygroscopic easy-to-dye crimped fiber of the embodiment is as follows:
1) the polyamide 56 melt and the polybutylene terephthalate melt are converged in a composite spinning assembly in a spinning manifold through respective melt pipelines, sprayed out through an eccentric composite spinneret plate, and cooled to form a primary yarn;
wherein, the proportion of the sheath-core components is accurately adjusted by a metering pump, the content of polyamide 56 in the sheath layer is 35 wt%, and the content of polybutylene terephthalate in the core layer is 65 wt%;
wherein the temperature of the spinning beam is 288 ℃, and the pressure of the spinning assembly of the spinning beam is 17 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain soft moisture-absorbing and easily-dyed crimped fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.7m/s, the temperature of the side-blown air is 26 ℃, and the humidity of the side-blown air is 73%.
The post-treatment comprises the following steps: and performing oiling treatment, stretching treatment, heat setting treatment and winding treatment on the as-spun yarn. The stretching treatment is secondary stretching, the total stretching multiple is 3.6 times, and the stretching temperature is 65 ℃; the temperature during the heat-setting treatment was 180 ℃ and the winding speed was 4400 m/min.
The preparation method of the melt of polyamide 56 in this example was: drying polyamide 56 resin (96% sulfuric acid with relative viscosity of 2.9 and water content of 600ppm) in a vacuum drum dryer at 85 ℃ for 35h, and heating to a molten state by using a first screw extruder to form a polyamide 56 melt; wherein the first screw extruder is heated in five zones, the temperature of the first zone is 243 ℃, the temperature of the second zone is 258 ℃, the temperature of the third zone is 269 ℃, the temperature of the fourth zone is 278 ℃, and the temperature of the fifth zone is 288 ℃.
The preparation method of the polybutylene terephthalate melt in this example is as follows: drying polybutylene terephthalate resin (with intrinsic viscosity of 0.8dL/g and water content of 90ppm) in a continuous hot air drying tower at the drying temperature of 110 ℃ for 30h, and then heating to a molten state by using a second screw extruder to form polybutylene terephthalate melt; wherein the second screw extruder is heated in five zones, the temperature of the first zone is 255 ℃, the temperature of the second zone is 275 ℃, the temperature of the third zone is 283 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 288 ℃.
The relative viscosity and intrinsic viscosity were measured as described in example 1.
Example 5
The preparation method of the soft hygroscopic easy-to-dye crimped fiber of the embodiment is as follows:
1) the polyamide 510 melt and the polyethylene terephthalate melt are converged in a composite spinning assembly in a spinning manifold through respective melt pipelines, sprayed out through a core-shifting composite spinneret plate, and cooled to form primary yarns;
wherein, the proportion of the sheath-core components is accurately adjusted by a metering pump, the content of polyamide 510 in the sheath layer is 50 wt%, and the content of polyethylene terephthalate in the core layer is 50 wt%;
wherein the temperature of the spinning beam is 280 ℃, and the pressure of the spinning assembly of the spinning beam is 13 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain soft moisture-absorbing and easily-dyed crimped fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.8m/s, the temperature of the side-blown air is 25 ℃, and the humidity of the side-blown air is 72%.
The post-treatment comprises the following steps: and performing oiling treatment, stretching treatment, heat setting treatment and winding treatment on the as-spun yarn. The stretching treatment is secondary stretching, the total stretching multiple is 2.5 times, and the stretching temperature is 70 ℃; the temperature during the heat-setting treatment was 160 ℃ and the winding speed was 4500 m/min.
The preparation method of the polyamide 510 melt in this example is as follows: drying polyamide 510 resin (96% sulfuric acid has a relative viscosity of 2.6 and a water content of 500ppm) in a vacuum drum dryer at 80 ℃ for 20h, and heating to a molten state by using a first screw extruder to form a polyamide 510 melt; wherein the first screw extruder is heated in five zones, the temperature of the first zone is 250 ℃, the temperature of the second zone is 255 ℃, the temperature of the third zone is 260 ℃, the temperature of the fourth zone is 265 ℃ and the temperature of the fifth zone is 270 ℃.
The preparation method of the polyethylene terephthalate melt in this example was: drying polyethylene terephthalate resin (with intrinsic viscosity of 0.65dL/g and water content of 80ppm) in a continuous hot air drying tower at 160 ℃ for 20h, and heating to a molten state by using a second screw extruder to form a polyethylene terephthalate melt; wherein the second screw extruder is heated in five zones, the temperature of the first zone is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 285 ℃.
The relative viscosity and intrinsic viscosity were measured as described in example 1.
Example 6
The preparation method of the soft hygroscopic easy-to-dye crimped fiber of the embodiment is as follows:
1) the polyamide 512 melt and the polyethylene glycol terephthalate melt are converged in a composite spinning assembly in a spinning manifold through respective melt pipelines, sprayed out through a core-shifting composite spinneret plate, and cooled to form primary yarns;
wherein, the proportion of the sheath-core components is accurately adjusted by a metering pump, the content of polyamide 512 in the sheath layer is 40 wt%, and the content of polyethylene terephthalate in the core layer is 60 wt%;
wherein the temperature of the spinning manifold is 285 ℃, and the pressure of the spinning assembly of the spinning manifold is 13 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain soft moisture-absorbing and easily-dyed crimped fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.9m/s, the temperature of the side-blown air is 24 ℃, and the humidity of the side-blown air is 75%.
The post-treatment comprises the following steps: and performing oiling treatment, stretching treatment, heat setting treatment and winding treatment on the as-spun yarn. The stretching treatment is secondary stretching, the total stretching multiple is 2.8 times, and the stretching temperature is 80 ℃; the temperature during the heat setting treatment was 180 ℃ and the winding speed was 4800 m/min.
The preparation method of the polyamide 512 melt in this example is as follows: drying polyamide 512 resin (96% sulfuric acid with relative viscosity of 2.7 and water content of 700ppm) in a vacuum drum dryer at 90 ℃ for 15h, and heating to a molten state by using a first screw extruder to form a polyamide 512 melt; wherein the first screw extruder is heated in five zones, the temperature of the first zone is 253 ℃, the temperature of the second zone is 260 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 275 ℃, and the temperature of the fifth zone is 280 ℃.
The preparation method of the polyethylene terephthalate melt in this example was: drying polyethylene terephthalate resin (with intrinsic viscosity of 0.67dL/g and water content of 90ppm) in a continuous hot air drying tower at 150 ℃ for 22h, and heating to a molten state by using a second screw extruder to form a polyethylene terephthalate melt; wherein the second screw extruder is heated in five zones, the temperature of the first zone is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 285 ℃.
The relative viscosity and intrinsic viscosity were measured as described in example 1.
Comparative example 1
The fiber of comparative example 1 was prepared as follows:
1) feeding the polyethylene glycol terephthalate melt into a single-component spinning assembly through a melt pipeline, extruding the polyethylene glycol terephthalate melt through a single-component spinneret plate, and cooling to form primary raw silk;
wherein the temperature of the spinning beam is 295 ℃, and the pressure of the spinning assembly of the spinning beam is 14 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.7m/s, the temperature of the side-blown air is 26 ℃, and the humidity of the side-blown air is 75%.
The post-treatment comprises the following steps: and (3) carrying out stretching treatment, heat setting treatment and winding treatment on the primary yarn. The stretching treatment is secondary stretching, the total stretching multiple is 3.0 times, and the stretching temperature is 90 ℃; the temperature during the heat-setting treatment was 130 ℃ and the winding speed was 4800 m/min.
The preparation method of the polyethylene terephthalate melt in this example was: drying polyethylene terephthalate resin (with intrinsic viscosity of 0.68dL/g and water content of 50ppm) in a continuous hot air drying tower at 130 ℃ for 28h, and heating to a molten state by using a screw extruder to form a polyethylene terephthalate melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 295 ℃.
The intrinsic viscosity was measured as described in example 1.
Comparative example 2
The fibers of comparative example 2 were prepared as follows:
1) the polyamide 6 melt and the polyethylene glycol terephthalate melt are converged in a composite spinning assembly in a spinning manifold through respective melt pipelines, sprayed out through a core-shifting composite spinneret plate, and cooled to form primary yarns;
wherein, the proportion of the sheath-core components is accurately adjusted by a metering pump, the content of polyamide 6 in the sheath layer is 40 wt%, and the content of polyethylene terephthalate in the core layer is 60 wt%;
wherein the temperature of the spinning manifold is 285 ℃, and the pressure of the spinning assembly of the spinning manifold is 11 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.8m/s, the temperature of the side-blown air is 26 ℃, and the humidity of the side-blown air is 65%.
The post-treatment comprises the following steps: and performing oiling treatment, stretching treatment, heat setting treatment and winding treatment on the as-spun yarn. The stretching treatment is secondary stretching, the total stretching multiple is 2.8 times, and the stretching temperature is 70 ℃; the temperature during the heat-setting treatment was 200 ℃ and the winding speed was 4400 m/min.
The preparation method of the polyamide 6 melt in this example was: drying polyamide 6 resin (96% sulfuric acid with relative viscosity of 2.7 and water content of 800ppm) in a vacuum drum dryer at 120 ℃ for 12h, and heating to a molten state by using a first screw extruder to form a polyamide 6 melt; wherein the first screw extruder is heated in five zones, the temperature of the first zone is 245 ℃, the temperature of the second zone is 256 ℃, the temperature of the third zone is 264 ℃, the temperature of the fourth zone is 275 ℃, and the temperature of the fifth zone is 290 ℃.
The preparation method of the polyethylene terephthalate melt in this example was: drying polyethylene terephthalate resin (with intrinsic viscosity of 0.65dL/g and water content of 70ppm) in a continuous hot air drying tower at 155 ℃ for 20h, and heating to a molten state by using a second screw extruder to form a polyethylene terephthalate melt; wherein the second screw extruder is heated in five zones, the temperature of the first zone is 260 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 290 ℃.
The relative viscosity and intrinsic viscosity were measured as described in example 1.
Comparative example 3
The fibers of comparative example 3 were prepared as follows:
1) the polyamide 66 melt and the polyethylene glycol terephthalate melt are converged in a composite spinning assembly in a spinning manifold through respective melt pipelines, sprayed out through a core-shifting composite spinneret plate, and cooled to form primary yarns;
wherein, the proportion of the sheath-core components is accurately adjusted by a metering pump, the content of polyamide 66 in the sheath layer is 30 wt%, and the content of polyethylene terephthalate in the core layer is 70 wt%;
wherein the temperature of the spinning beam is 290 ℃, and the pressure of the spinning assembly of the spinning beam is 15 MPa.
2) Carrying out post-treatment on the primary raw silk to obtain fibers;
wherein the cooling treatment is side-blown cooling, the air speed of the side-blown air is 0.7m/s, the temperature of the side-blown air is 22 ℃, and the humidity of the side-blown air is 60%.
The post-treatment comprises the following steps: and performing oiling treatment, stretching treatment, heat setting treatment and winding treatment on the as-spun yarn. The stretching treatment is secondary stretching, the total stretching multiple is 2.5 times, and the stretching temperature is 75 ℃; the temperature at the time of heat setting was 170 ℃ and the winding speed was 4600 m/min.
The preparation method of the polyamide 66 melt in the embodiment comprises the following steps: drying polyamide 66 resin (96% sulfuric acid with relative viscosity of 2.8 and water content of 700ppm) in a vacuum drum dryer at 115 ℃ for 24h, and heating to a molten state by using a first screw extruder to form a polyamide 66 melt; wherein the first screw extruder is heated in five zones, the temperature of the first zone is 245 ℃, the temperature of the second zone is 260 ℃, the temperature of the third zone is 270 ℃, the temperature of the fourth zone is 280 ℃, and the temperature of the fifth zone is 290 ℃.
The preparation method of the polyethylene terephthalate melt in this example was: drying polyethylene terephthalate resin (with intrinsic viscosity of 0.67dL/g and water content of 70ppm) in a continuous hot air drying tower at 145 ℃ for 30h, and heating to a molten state by using a second screw extruder to form a polyethylene terephthalate melt; wherein the second screw extruder is heated in five zones, the temperature of the first zone is 255 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 295 ℃.
The relative viscosity and intrinsic viscosity were measured as described in example 1.
Test examples
The fibers of examples 1-6 above and the fibers of comparative examples 1-3 were tested as follows, and the results are shown in Table 1.
1. Breaking strength, elongation at break, modulus:
determination of breaking Strength and elongation at Break according to the testing method of GB/T14334-: applying a pretension of 0.05 +/-0.005 cN/dtex, a holding distance of 500mm and a drawing speed of 500 mm/min.
Modulus-100 strength at break corresponding to 1% elongation at break.
2. Moisture regain:
the determination method of the moisture regain comprises the following steps: and (3) putting the washed fiber in a loose state into an oven for drying, putting the dried fiber sample in standard atmosphere specified in GB/T6529 for debugging and balancing, and humidifying for 2 h. And washing the humidity-adjusted sample, and measuring the moisture regain, wherein the moisture regain measuring method is executed according to GB/T6503, the drying temperature of an oven is 105 ℃, and the drying time is 1 h.
3. Dye uptake
The method for measuring the dye-uptake rate comprises the following steps: the change in dye liquor concentration before and after dyeing was measured with a spectrophotometer.
Dye uptake (%) - (A)0-At)/A0*100％
Wherein A is0The absorbance value of the characteristic absorption peak of the dye before treatment, AtIs the absorbance value of the dye at the treatment time t.
This test example uses the fiber hose tapes prepared from the fibers of examples and comparative examples, which were dyed with acid dyes and disperse dyes, respectively, to measure the dye uptake.
4. Tensile elastic recovery:
the untreated filaments were measured using an electronic single yarn strength tester YG061 at an ambient temperature of 23 ℃ and a humidity of 65%. The sample holding distance was 250mm, the drawing speed was 500mm/min, and the fixed elongation values were 5%, 10%, and 15% of the holding distance, respectively.
The treated filaments (100 ℃, 15min) were treated with a fiber electron brute force instrument LLY06 at an ambient temperature of 23 ℃ and a humidity of 65%. The sample holding distance was 30mm, the drawing speed was 60mm/min, and the fixed elongation values were 50%, 100%, and 150% of the holding distance, respectively.
Elastic recovery rate ((L-L)1)/(L-L0))*100％
Wherein L is0Is the original length of the sample, L is the length of the sample after stretching to a fixed extension, L1The length of the sample after reset.
As can be seen from Table 1: the softness, hygroscopicity and three-dimensional crimpability of the fiber prepared by the method are obviously improved, and the dyeing of acid dye and disperse dye can be completed at low temperature.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (14)
1. The soft moisture-absorption dyeable crimped fiber is characterized by comprising the following components in percentage by mass: polyamide 5X 10-50%, polyester 50-90%; the polyamide 5X is formed by polymerizing 1, 5-pentanediamine and dibasic acid, wherein the dibasic acid comprises aliphatic dibasic acid of C6-20; the polyester is selected from one or more of polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate and modified polyester; the initial modulus of the soft hygroscopic easily-dyed crimped fiber is 20-38.6 cN/dtex;
the dyeing dye uptake of the soft hygroscopic easy-to-dye crimped fiber acid dye is 78-92%, and the dyeing temperature of the acid dye is 50-90 ℃.
2. A soft, absorbent and dyeable crimped fiber according to claim 1, wherein the soft, absorbent and dyeable crimped fiber has a sheath-core structure, the polyamide is a sheath material, and the polyester is a core material; the skin-core structure comprises a positive core structure and an eccentric core structure.
3. A soft, absorbent, dyeable, crimped fiber according to claim 2, wherein the sheath-core structure is a bias core structure.
4. A soft hygroscopic dyeable crimped fiber according to claim 3, wherein the polyamide 5X is selected from one or more of polyamide 56, polyamide 510 or polyamide 512.
5. A soft, absorbent, dyeable, crimped fiber according to any one of claims 1 to 4, wherein the soft, absorbent, dyeable, crimped fiber has a denier of from 10 to 1000 dtex.
6. A soft, moisture-sensitive, dyeable, crimped fiber according to any of claims 1 to 4, wherein the soft, moisture-sensitive, crimped fiber has a tenacity at break of from 2.5 to 7cN/dtex and an elongation at break of from 20 to 60%.
7. A soft, hygroscopic, dyeable, crimped fiber according to any one of claims 1 to 4, wherein the moisture regain of the soft, hygroscopic, dyeable, crimped fiber is from 1 to 3%.
8. A soft, absorbent, dyeable, crimped fiber according to any one of claims 1 to 4, wherein the soft, absorbent, dyeable, crimped fiber has an untreated elastic recovery of 85 to 100% and a treated elastic recovery of 85 to 100%.
9. A soft, hygroscopic, easily dyeable crimped fiber according to any one of claims 1 to 4, wherein the soft, hygroscopic, easily dyeable crimped fiber has a disperse dye dyeing degree of 85 to 100% and a disperse dye dyeing temperature of 80 to 130 ℃.
10. A process for preparing soft, hygroscopic, easily dyeable crimped fiber according to any one of claims 1 to 9, comprising the steps of:
1) after the polyamide 5X melt and the polyester melt are converged in a composite spinning assembly in a spinning manifold, the melt is sprayed out through a core composite spinneret plate, and the raw silk is generated after cooling treatment;
2) carrying out post-treatment on the as-spun yarn to obtain the soft moisture-absorbing and easily-dyed crimped fiber;
wherein the post-treatment comprises stretching treatment, the temperature of the stretching treatment is 50-200 ℃, the stretching treatment is at least two-stage stretching, and the total stretching multiple of the stretching treatment is 1.5-5.0.
11. The method for preparing soft moisture-absorbing and easy-dyeing crimped fiber according to claim 10, wherein the post-treatment further comprises heat setting treatment and winding treatment, the temperature of the heat setting treatment is 100-200 ℃, and the speed of the winding treatment is 2000-5500 m/min.
12. The method of claim 10, wherein a first heat treatment is performed on polyamide 5X using a first screw extruder to obtain a melt of polyamide 5X; carrying out second heat treatment on the polyester by using a second screw extruder to obtain a polyester melt;
the working parameters of the first screw extruder for carrying out the first heat treatment are as follows: a five-zone heating mode, wherein the temperature of the first zone is 200-260 ℃, the temperature of the second zone is 230-280 ℃, the temperature of the third zone is 240-290 ℃, the temperature of the fourth zone is 260-300 ℃, and the temperature of the fifth zone is 270-310 ℃;
the working parameters of the second screw extruder for carrying out the second heat treatment are as follows: a five-zone heating mode, wherein the temperature of the first zone is 200-260 ℃, the temperature of the second zone is 230-280 ℃, the temperature of the third zone is 240-290 ℃, the temperature of the fourth zone is 260-300 ℃, and the temperature of the fifth zone is 280-300 ℃;
in the first screw extruder and the second screw extruder, the temperature of the second zone is higher than the temperature of the first zone, and the temperature of the third zone, the temperature of the fourth zone and the temperature of the fifth zone are respectively higher than the temperature of the first zone and/or the temperature of the second zone.
13. The method of claim 10, wherein the soft, hygroscopic, easily dyeable crimped fiber is produced by,
the temperature of the spinning manifold is 220-320 ℃, and the pressure of the composite spinning assembly is 10-30 MPa.
14. The method of claim 10, wherein the cooling process is cross-blow cooling, the air velocity of the cross-blow is 0.5-1.3m/s, the temperature of the cross-blow is 14-30 ℃, and the humidity of the cross-blow is 60-80%.
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| CN112680826A (en) * | 2019-10-18 | 2021-04-20 | 上海凯赛生物技术股份有限公司 | Polyamide sea-island fiber and preparation method and application thereof |
| CN111519274B (en) * | 2020-01-20 | 2023-01-06 | 浙江新维狮合纤股份有限公司 | Production process of superfine fiber with super-soft bi-component sheath-core structure and superfine fiber thereof |
| CN115679475A (en) * | 2021-07-21 | 2023-02-03 | 中国科学院化学研究所 | Composite fiber based on PA56 and preparation method and application thereof |
| CN115787131A (en) * | 2022-12-23 | 2023-03-14 | 福建长源纺织有限公司 | Sheath-core polyamide-polyester composite fiber and preparation method thereof |
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